A hydrmetallurgical study based on the extraction of Zn and Pb from a Nigerian sphalerite mineral leached with 4 M hydrochloric acid has been undertaken. Triphenylphosphite (TPP) has proved to be very effective for the extraction of zinc. With 2 M TPP and at ambient temperature of 25±2°C; 35.71% and 66.7% of Pb and Zn were extracted, respectively, into the organic phase within 60 min. The recovery rates of 93.27% and 91.16% from the organic phase were obtained after de-extraction with 6 M HCl for Pb and Zn, respectively. Finally lead has been successfully separated from zinc by the cementation of the former with zinc metal. The mechanism of extraction appeared to be chelate formation and ion exchange.